← Back to Patent Explorer
US5405592A Expired / Lapsed US ⏱️ 0.0 years remaining

Non-densified silicon nitride beta-phase material

Assignee: Mid-America Commercialization Corp
•
Filing: 1992-10-20
•
Granted: 1995-04-11
•
Expires: 2012-10-20
📄 Original PDF 🌐 Google Patents 🔄 Sync Now

Abstract

Abstract A silicon-nitride beta-phase material including a non-densified structure of beta silicon nitride crystals having appreciable strength without any significant amount of liquid forming agents is made by comminuting a slurry including a mixture of silicon powder and water to form non-oxidized surfaces on the silicon powder and to allow chemical reaction between the silicon and the water, reducing the water content of the reacted slurry to a degree sufficient to form a resultant dry mass, nitriding the dry mass by exposure to a nitriding gas including at least nitrogen to form a mass of alpha-phase silicon nitride, and converting the resultant silicon nitride mass at a conversion temperature of from about 1450° C. to about 2100° C. to convert the silicon nitride from an alpha-phase material to a non-densified beta phase silicon nitride material.

Inventors

  • 👤 James P. Edler
  • 👤 Bohdan Lisowsky

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-04 13:14
CPC Classifications
C; C01; C01B; C01B21/00; C01B21/06; C01B21/068; C01B21/0687; C04; C04B; C04B35/00; C04B35/515; C04B35/58; C04B35/584; C04B35/591

Claims Analysis

Total Claims: 23
Claim 1
Independent Claim 191 words
A silicon nitride beta-phase material comprising a structure of beta-phase silicon nitride crystals and at least one nitriding agent having a bulk density of less than about 3.2 g/cm 3 , an apparent porosity of at least about 10%, and less than 10 weight percent alpha-phase silicon nitride without any significant amounts of densification aids made by (a) comminuting a slurry including a mixture consisting essentially of (i) silicon-containing powder, (ii) water, and (iii) at least one nitriding agent, said comminuting being performed to form non-oxidized surfaces on the silicon powder and to allow chemical reaction between the silicon and the water; (b) reducing the water content of the reacted slurry to a degree sufficient to form a resultant dry mass; (c) nitriding the dry mass by exposure to a nitriding gas including at least nitrogen to form a mass of substantially alpha-phase silicon nitride; and (d) converting the resultant silicon nitride mass at a conversion temperature of from about 1450° C. to about 2100° C. for a sufficient length of time to convert the silicon nitride from an alpha-phase material to a beta-phase material having at least one nitriding agent.
Claim 2
Dependent Claim 191 words
A silicon nitride beta-phase material comprising a structure of beta-phase silicon nitride crystals and at least one nitriding agent having a bulk density of less than about 3.2 g/cm 3 , an apparent porosity of at least about 10%, and less than 10 weight percent alpha-phase silicon nitride without any significant amounts of densification aids made by (a) comminuting a slurry including a mixture consisting essentially of (i) silicon-containing powder, (ii) water, and (iii) at least one nitriding agent, said comminuting being performed to form non-oxidized surfaces on the silicon powder and to allow chemical reaction between the silicon and the water; (b) reducing the water content of the reacted slurry to a degree sufficient to form a resultant dry mass; (c) nitriding the dry mass by exposure to a nitriding gas including at least nitrogen to form a mass of substantially alpha-phase silicon nitride; and (d) converting the resultant silicon nitride mass at a conversion temperature of from about 1450° C. to about 2100° C. for a sufficient length of time to convert the silicon nitride from an alpha-phase material to a beta-phase material having at least one nitriding agent.
Claim 3
Dependent Claim 85 words
The silicon nitride beta-phase material of claim 1, wherein the at least one nitriding agent is selected from the group consisting of iron oxides, lead oxides, nickel carbonyl, nickel oxides, silicon carbide, graphite, carbon aluminum oxides, CoO, CaF, Li 2 O, Na 2 O, K 2 O, BaO, BN, albite (NaAlSi 3 O 8 ), orthclase (KAlSi 3 O 8 ) , anorthite (CaAl 2 Si 2 O 8 ) , nepheline syenite, talc, borax, soda ash, alpha-phase Si 3 N 4 and mixtures thereof.
Claim 4
Dependent Claim 49 words
A silicon nitride beta-phase material comprising a structure of beta-phase silicon nitride crystals having a bulk density of less than about 3.2 g/cm 3 , less than 10 weight percent alpha-phase silicon nitride, and an apparent porosity of at least about 10% without any significant amounts of densification aids.
Claim 5
Dependent Claim 49 words
A silicon nitride beta-phase material comprising a structure of beta-phase silicon nitride crystals having a bulk density of less than about 3.2 g/cm 3 , less than 10 weight percent alpha-phase silicon nitride, and an apparent porosity of at least about 10% without any significant amounts of densification aids.
Claim 6
Dependent Claim 20 words
The silicon nitride beta-phase material of claim 3 having a bulk density of less than about 2.8 g/cm 3 .
Claim 7
Dependent Claim 33 words
The silicon nitride beta-phase material of claim 3 having a hardness of at least 100 Knoop hardness number measured with a 500 gram load on a polished surface using a Tukon hardness tester.
Claim 8
Dependent Claim 36 words
The silicon nitride beta-phase material of claim 3 having a hardness of from about 400 to about 800 Knoop hardness number measured with a 500 gram load on a polished surface using a Tukon hardness tester.
Claim 9
Dependent Claim 17 words
The silicon nitride beta-phase material of claim 3 having a hardness of at least Rockwell A 20.
Claim 10
Dependent Claim 19 words
The silicon nitride beta-phase material of claim 3 having less than about 5 weight percent alpha-phase silicon nitride present.
Claim 11
Dependent Claim 22 words
The silicon nitride beta-phase material of claim 3 having equiaxed beta-phase silicon nitride grain size from about 0.1 to about 20 microns.
Claim 12
Dependent Claim 22 words
The silicon nitride beta-phase material of claim 3 having equiaxed beta-phase silicon nitride grain size from about 0.5 to about 5 microns.
Claim 13
Dependent Claim 19 words
The silicon nitride beta-phase material of claim 3 having pores from about 0.1 to about 50 microns in size.
Claim 14
Dependent Claim 19 words
The silicon nitride beta-phase material of claim 3 having pores from about 1 to about 10 microns in size.
Claim 15
Dependent Claim 32 words
The silicon nitride beta-phase material of claim 3 exhibiting not more than a 10,000 pounds per square inch decrease in hot flexure strength over about a 100° C. increase in test temperature.
Claim 16
Dependent Claim 25 words
The silicon nitride beta-phase material of claim 3 wherein liquid forming agents are present in less than 2 volume percent of the silicon nitride material.
Claim 17
Dependent Claim 25 words
The silicon nitride beta-phase material of claim 3 wherein liquid forming agents are present in less than 1 volume percent of the silicon nitride material.
Claim 18
Dependent Claim 26 words
The silicon nitride beta-phase material of claim 3 having at least 75% equiaxed beta-phase silicon nitride grains in size from about 0.1 to about 20 microns.
Claim 19
Dependent Claim 26 words
The silicon nitride beta-phase material of claim 3 having at least 50% equiaxed beta silicon nitride grains in size from about 0.1 to about 20 microns.
Claim 20
Dependent Claim 25 words
The silicon nitride beta-phase material of claim 3 wherein at least 75% of the pores are from about 0.1 to about 50 microns in size.
Claim 21
Dependent Claim 25 words
The silicon nitride beta-phase material of claim 3 wherein at least 50% of the pores are from about 0.1 to about 50 microns in size.
Claim 22
Dependent Claim 19 words
The silicon nitride beta-phase material of claim 3 wherein the material is in the form of a compacted article.
Claim 23
Dependent Claim 19 words
The silicon nitride beta-phase material of claim 1, wherein the converting step is conducted for at least 0.3 hours.

References Cited (Backward Citations)

US3950464A Cited
US4354990A Cited
US4492665A Cited
US4888142A Cited
US5002907A Cited
US4943401A Cited
US4919689A Cited
US5114693A Cited
US5156830A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1998-04-10 1998-10-10 1999-04-11 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 2002-04-10 2002-10-10 2003-04-11 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2006-04-10 2006-10-10 2007-04-11 $7700.00 Window Closed / Lapsed

Assigned Categories & Tags

No categories assigned to this patent yet.

Assign Category Tag